2H-1-Benzopyran-2-methanol, alpha,alpha'-[[(phenylmethyl)imino]bis(methylene)]bis[6-fluoro-3,4-dihydro-, (alphaR,alpha'R,2R,2'S)-rel-

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

01 October 2015 - 22 January 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2016

Report date:

2016

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

Test guideline 3

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Reference substance name:

2H-1-Benzopyran-2-methanol, alpha,alpha'-[[(phenylmethyl)imino]bis(methylene)]bis[6-fluoro-3,4-dihydro-, (alphaR,alpha'R,2R,2'S)-rel-

EC Number:

618-043-4

Cas Number:

876666-07-8

Molecular formula:

C29H31F2NO4

IUPAC Name:

2H-1-Benzopyran-2-methanol, alpha,alpha'-[[(phenylmethyl)imino]bis(methylene)]bis[6-fluoro-3,4-dihydro-, (alphaR,alpha'R,2R,2'S)-rel-

Test material form:

solid: particulate/powder

Details on test material:

- Name of test material (as cited in study report): JNJ-17303806-AAA (T001586)
- Physical state: solid, powder
- Appearance: white, beige

Specific details on test material used for the study:

- Batch n°: I15EB1984
- Analytical purity: 99.9% (base titration)
- Expiration date: 08 November 2016
- Storage condition: at room temperature

Results and discussion

Melting / freezing point

Key result

Melting / freezing pt.:

121.3 °C

Atm. press.:

1 013.25 hPa

Decomposition:

yes

Decomp. temp.:

> 200 °C

Remarks on result:

other: A dark brown molten residue remained after the preliminary and main test (up to 374°C), indicating reaction and/or decomposition.

Any other information on results incl. tables

Preliminary test

From the TGA curve it could be derived that the weight of the sample decreased significantly at 325°C. At 374°C the sample weight has decreased by 25%. After the experiment, a dark brown black molten residue remained in the sample container (original colour: white). The change of the colour indicated reaction and/or decomposition of the test item.

Main tests

In order to determine the melting more precisely, the DSC curve with a heating rate of 20°C/min showed an endothermic peak between 100°C and 150°C. The extrapolated onset temperature of the peak was 121.19°C. The effect was most likely obtained due to melting. An exothermic peak was observed starting at 200°C due to reaction and/or decomposition of the test item. After the experiment, a dark brown molten residue remained. To investigate the melting peak between 100°C and 150°C, a repeated heating cycle was applied. The extrapolated onset temperature of the melting peak was 121.16°C. In a further heating cycle, the extrapolated onset temperature of the melting peak was 121.52°C. After the experiment, a white molten residue remained in the sample container. The result demonstrated that the endothermic effect was due to melting of the test item.

The melting temperature of T001586 was determined as the average melting temperature obtained from Experiment 1, Experiment 2 and Experiment 3 and equals 121.3°C (394.4K).

Applicant's summary and conclusion

Conclusions:

The melting temperature of JNJ-17303806-AAA (T001586) was determined to be 121.3°C (394.4K) by using DSC.